US20040008814A1 - Robot compatible crystal worksite suite - Google Patents

Robot compatible crystal worksite suite Download PDF

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Publication number
US20040008814A1
US20040008814A1 US10/349,234 US34923403A US2004008814A1 US 20040008814 A1 US20040008814 A1 US 20040008814A1 US 34923403 A US34923403 A US 34923403A US 2004008814 A1 US2004008814 A1 US 2004008814A1
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Prior art keywords
dewar
magazine
worksite
flask
rim
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US10/349,234
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US6925815B2 (en
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Richard Shafer
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Oceaneering International Inc
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Assigned to OCEANEERING INTERNATIONAL INC. reassignment OCEANEERING INTERNATIONAL INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: NIENABER, TERRENCE J., ROBERTSON, WILLIAM C., SHAFER, RICHARD E.
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Assigned to WELLS FARGO BANK, NATIONAL ASSOCIATION reassignment WELLS FARGO BANK, NATIONAL ASSOCIATION SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GRAYLOC PRODUCTS, L.L.C., MARINE PRODUCTION SYSTEMS, LTD., OCEANEERING CANADA LIMITED, OCEANEERING INTERNATIONAL, INC.
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials

Definitions

  • the present invention is directed to a suite of apparatus used in handling crystals for x-ray crystallographic analysis. More specifically, the suite of apparatus includes a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals.
  • U.S. Pat. No. 6,408,047 discloses a method of performing x-ray crystallography on samples by using a robot to transfer the samples to a goniometer.
  • This patent is incorporated herein by reference.
  • the patent discloses the general system that the present invention is directed to but does not disclose a worksite suite as disclosed herein.
  • U.S. Pat. No. 6,404,849 discloses a method and apparatus for mounting a crystal sample for x-ray crystallographic analysis. This patent is incorporated herein by reference. The patent discloses the general system that the present invention is directed to but does not disclose a worksite suite as disclosed herein.
  • the present invention is directed to a robot compatible crystal worksite suite comprising a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals.
  • FIG. 1 is a magazine of the present invention
  • FIG. 2 is an exploded view of a magazine of the present invention
  • FIG. 3 is a top view of a magazine of the present invention.
  • FIG. 4 is a cross-sectional view of a magazine of the present invention along line 4 - 4 of FIG. 3;
  • FIG. 5 is a top view of a magazine tongs that is part of the worksite suite of the present invention.
  • FIG. 6 is a side view of the magazine tongs in FIG. 5;
  • FIG. 7 is a shipping rack that holds five magazines of the present invention.
  • FIG. 8 is a worksite dewar
  • FIG. 9 is a partial cross-section of the dewar
  • FIG. 10 is the dewar with a programmed controller
  • FIG. 11 is a top view of the worksite dewar that has no magazines inside;
  • FIG. 12 is a top view of the worksite dewar that has five (5) magazines inside;
  • FIG. 13 is a cryo-pin tongs that removes cryo-pins from a magazine manually and is part of the worksite suite of the present invention.
  • the central component of the suite of apparatus of the present invention used in handling crystals for x-ray crystallographic analysis is a multi-position magazine.
  • the magazine is used for precisely locating, protecting and transferring batches of crystals that require cryogenic storage and handling.
  • the magazine 10 is constructed from two parts, as shown in FIG. 1 and FIG. 2.
  • the top part 12 of magazine 10 has a plurality of cylinders 14 , specifically shown are twelve ( 12 ) cylinders; however the exact number may vary.
  • the cylinders 14 are held by an outer member 15 that is essentially configured as a circle.
  • the lower part 16 of magazine 10 has the same number of location bosses 18 as cylinders 14 that are positioned to be centered in the corresponding cylinder. In each location boss 18 is a magnet 20 .
  • the strong magnets 20 are held in place with epoxy to hold the cryo-pin 30 , a product of Hampton Research having a ferrous base 34 (see FIG. 4), securely on the location bosses 18 .
  • the magnets 20 also hold the magazine 10 securely on a ferrous work surface during crystal manipulation.
  • the upper part 12 and lower part 16 of magazine 10 are held together with epoxy and pressed spring pins 24 .
  • the outer member 15 conforms to surface of the cylinders 14 to provide guides 17 the gross location of the magazine 10 .
  • a member 19 is in a form to provide tabs 21 for the forceps grasping tool 40 and a slot 23 for a locking pin, described hereinafter.
  • the magazine 10 described in FIGS. 1 - 4 provides a device for protecting and transferring twelve crystals each mounted on a cryo-pin 30 .
  • the cryo-pins 30 that hold the frozen crystals, are seated in the cylinders 14 of the magazine 10 as shown in FIG. 4.
  • the cylinders 14 hold liquid nitrogen and keep the cryo-pins 30 submerged in the liquid nitrogen while the magazine 10 is transfer from one dewar to another.
  • the cylinders 14 also protect the crystals and pins 30 , which are held to the boss 18 on the bottom part 16 of the magazine 10 by the magnets 20 .
  • the magazine 10 is handled using a grasping tool or magazine tongs 40 that utilize a “dumbbell” shaped tip 42 attached to the end of forceps 44 (FIGS. 5 and 6).
  • the tips 42 grasp the magazine 10 via slotted tabs 21 at the top edge of the magazine 10 , as shown in FIG. 3. Since the magazine 10 is typically submerged in liquid nitrogen, the magazine tongs 40 allow the user to remove the magazine from one dewar to another.
  • the typical dewar of the prior art has a rack with a number of rack plates each spaced by threaded standoff members.
  • the rack 50 shown in FIG. 7 is designed to be compatible with the magazines 10 and the suite of the present invention thus having six plates 52 .
  • the plates 52 are made from martensitic stainless steel that allows the magazine 10 to be held in place by the magnets 20 .
  • the threaded standoff members 54 are configured to provide the spacing between plates 52 to place a magazine 10 on each plate 52 and provide a guide for the gross location of the magazine 10 on the plate 52 .
  • a retaining bar 56 fits in slot 23 of magazines 10 (FIG. 3) to securely hold the magazine 10 on the plate 52 .
  • the retaining bar 56 is held in position by passing through holes in plates 52 and secured by a magnet 58 .
  • a support rod 59 is attachable to the top plate 52 to place the five magazines into or remove the magazines from a dewar.
  • the worksite dewar 60 provides a staging area for the crystallography system.
  • the dewar 60 is placed in a mounting fixture 62 that is precisely calibrated with the robotic arm of a robot system.
  • a condensation catch pan 64 is at the bottom of the dewar 60 .
  • the dewar 60 has a lid 66 .
  • the dewar is a double wall flask 68 with a vacuum between inner wall 67 and outer wall 69 .
  • the flask 68 is capable of holding liquid nitrogen.
  • On the outside of the flask 68 is insulation 70 .
  • At the upper portion of the flask 68 is a rim insulator 72 .
  • a heater 75 is mounted to the rim 77 to heat the rim 77 but is insulated from the flask 68 .
  • the heater 75 minimizes condensation on the rim and prevents the freezing of any condensation that does form on the rim 77 that would prevent the lid 66 from opening.
  • the worksite dewar lid actuator assembly 65 is connected to a programmable controller 80 that may be separate from or part of the robot system.
  • the actuator assembly 65 is comprised of a commercial linear actuator attached to the outboard end of the lid hinge 67 , beyond the lid hinge pin.
  • the actuator assembly 65 also includes micro switches which provide interlocks for both robot and dewar lid operation.
  • the controller 80 will open the lid 66 before the robotic arm enters the dewar 60 to remove or return a crystal to a magazine in the dewar 60 .
  • the worksite dewar 60 holds five magazines 10 .
  • the floor of flask 68 has a precision mounting plate 81 which has twenty alignment pins 82 , four for each magazine for the course alignment of a magazine 10 and ten alignment pins 84 for the fine alignment of each magazine 10 .
  • the dewar 60 has a liquid cryogen, liquid nitrogen, inlet 88 on the side of the dewar 60 . As shown in FIG. 12, five magazines 10 are placed in the working dewar 60 , containing a total of sixty samples of crystals to be tested by x-ray crystallography.
  • Pin tongs 90 are part of the suite of the present invention since there are occasions when the cryo-pins 30 are handled manually.

Abstract

The present invention is directed to a robot compatible crystal worksite suite comprising a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals.

Description

    RELATED APPLICATION
  • This application is based on provisional application No. 60/350,920, filed Jan. 23, 2002, entitled “Crystal Carrier Magazine System for Use in Crystallography Applications”.[0001]
    • FIELD OF THE INVENTION
  • The present invention is directed to a suite of apparatus used in handling crystals for x-ray crystallographic analysis. More specifically, the suite of apparatus includes a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals. [0002]
    • BACKGROUND OF THE INVENTION
  • U.S. Pat. No. 6,408,047 discloses a method of performing x-ray crystallography on samples by using a robot to transfer the samples to a goniometer. This patent is incorporated herein by reference. The patent discloses the general system that the present invention is directed to but does not disclose a worksite suite as disclosed herein. [0003]
  • U.S. Pat. No. 6,404,849 discloses a method and apparatus for mounting a crystal sample for x-ray crystallographic analysis. This patent is incorporated herein by reference. The patent discloses the general system that the present invention is directed to but does not disclose a worksite suite as disclosed herein. [0004]
  • While both patents disclose the general environment of the present invention, the present invention is directed to a worksite suite suitable for use when using a robot to provide the high throughput, automated crystallography methods disclosed in the patents. [0005]
    • SUMMARY OF THE INVENTION
  • The present invention is directed to a robot compatible crystal worksite suite comprising a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals.[0006]
    • BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 is a magazine of the present invention; [0007]
  • FIG. 2 is an exploded view of a magazine of the present invention; [0008]
  • FIG. 3 is a top view of a magazine of the present invention; [0009]
  • FIG. 4 is a cross-sectional view of a magazine of the present invention along line [0010] 4-4 of FIG. 3;
  • FIG. 5 is a top view of a magazine tongs that is part of the worksite suite of the present invention; [0011]
  • FIG. 6 is a side view of the magazine tongs in FIG. 5; [0012]
  • FIG. 7 is a shipping rack that holds five magazines of the present invention; [0013]
  • FIG. 8 is a worksite dewar; [0014]
  • FIG. 9 is a partial cross-section of the dewar; [0015]
  • FIG. 10 is the dewar with a programmed controller; [0016]
  • FIG. 11 is a top view of the worksite dewar that has no magazines inside; [0017]
  • FIG. 12 is a top view of the worksite dewar that has five (5) magazines inside; and [0018]
  • FIG. 13 is a cryo-pin tongs that removes cryo-pins from a magazine manually and is part of the worksite suite of the present invention.[0019]
    • DESCRIPTION OF THE INVENTION
  • The central component of the suite of apparatus of the present invention used in handling crystals for x-ray crystallographic analysis is a multi-position magazine. The magazine is used for precisely locating, protecting and transferring batches of crystals that require cryogenic storage and handling. The [0020] magazine 10 is constructed from two parts, as shown in FIG. 1 and FIG. 2. The top part 12 of magazine 10 has a plurality of cylinders 14, specifically shown are twelve (12) cylinders; however the exact number may vary. The cylinders 14 are held by an outer member 15 that is essentially configured as a circle. The lower part 16 of magazine 10 has the same number of location bosses 18 as cylinders 14 that are positioned to be centered in the corresponding cylinder. In each location boss 18 is a magnet 20. The strong magnets 20 are held in place with epoxy to hold the cryo-pin 30, a product of Hampton Research having a ferrous base 34 (see FIG. 4), securely on the location bosses 18. The magnets 20 also hold the magazine 10 securely on a ferrous work surface during crystal manipulation. The upper part 12 and lower part 16 of magazine 10 are held together with epoxy and pressed spring pins 24. Referring now to FIG. 3, the outer member 15 conforms to surface of the cylinders 14 to provide guides 17 the gross location of the magazine 10. On one surface of outer member 15, a member 19 is in a form to provide tabs 21 for the forceps grasping tool 40 and a slot 23 for a locking pin, described hereinafter.
  • The [0021] magazine 10 described in FIGS. 1-4 provides a device for protecting and transferring twelve crystals each mounted on a cryo-pin 30. The cryo-pins 30, that hold the frozen crystals, are seated in the cylinders 14 of the magazine 10 as shown in FIG. 4. The cylinders 14 hold liquid nitrogen and keep the cryo-pins 30 submerged in the liquid nitrogen while the magazine 10 is transfer from one dewar to another. The cylinders 14 also protect the crystals and pins 30, which are held to the boss 18 on the bottom part 16 of the magazine 10 by the magnets 20.
  • The [0022] magazine 10 is handled using a grasping tool or magazine tongs 40 that utilize a “dumbbell” shaped tip 42 attached to the end of forceps 44 (FIGS. 5 and 6). The tips 42 grasp the magazine 10 via slotted tabs 21 at the top edge of the magazine 10, as shown in FIG. 3. Since the magazine 10 is typically submerged in liquid nitrogen, the magazine tongs 40 allow the user to remove the magazine from one dewar to another. The typical dewar of the prior art has a rack with a number of rack plates each spaced by threaded standoff members. The rack 50 shown in FIG. 7 is designed to be compatible with the magazines 10 and the suite of the present invention thus having six plates 52. The plates 52 are made from martensitic stainless steel that allows the magazine 10 to be held in place by the magnets 20. The threaded standoff members 54 are configured to provide the spacing between plates 52 to place a magazine 10 on each plate 52 and provide a guide for the gross location of the magazine 10 on the plate 52. A retaining bar 56 fits in slot 23 of magazines 10 (FIG. 3) to securely hold the magazine 10 on the plate 52. The retaining bar 56 is held in position by passing through holes in plates 52 and secured by a magnet 58. A support rod 59 is attachable to the top plate 52 to place the five magazines into or remove the magazines from a dewar.
  • Reference is made to U.S. Pat. Nos. 6,408,047 and 6,494,849, both of which are directed to providing a method of performing x-ray crystallography on samples using a robot or robotic arm. The [0023] magazines 10 of the present invention are specially suited and compatible to be used in such a system. The worksite suite of the present invention provides for high volume of crystal samples to be tested while lessening the need for human intervention.
  • Another central component of the worksite suite of the present invention is the [0024] worksite dewar 60. Now referring to FIG. 8, the worksite dewar 60 provides a staging area for the crystallography system. The dewar 60 is placed in a mounting fixture 62 that is precisely calibrated with the robotic arm of a robot system. A condensation catch pan 64 is at the bottom of the dewar 60. The dewar 60 has a lid 66. The dewar is a double wall flask 68 with a vacuum between inner wall 67 and outer wall 69. The flask 68 is capable of holding liquid nitrogen. On the outside of the flask 68 is insulation 70. At the upper portion of the flask 68 is a rim insulator 72. A heater 75 is mounted to the rim 77 to heat the rim 77 but is insulated from the flask 68. The heater 75 minimizes condensation on the rim and prevents the freezing of any condensation that does form on the rim 77 that would prevent the lid 66 from opening.
  • Referring to FIG. 10, the worksite dewar [0025] lid actuator assembly 65, is connected to a programmable controller 80 that may be separate from or part of the robot system. The actuator assembly 65 is comprised of a commercial linear actuator attached to the outboard end of the lid hinge 67, beyond the lid hinge pin. The actuator assembly 65 also includes micro switches which provide interlocks for both robot and dewar lid operation. When part of the robot system, the controller 80 will open the lid 66 before the robotic arm enters the dewar 60 to remove or return a crystal to a magazine in the dewar 60. As shown in FIGS. 11 and 12, the worksite dewar 60 holds five magazines 10. The floor of flask 68 has a precision mounting plate 81 which has twenty alignment pins 82, four for each magazine for the course alignment of a magazine 10 and ten alignment pins 84 for the fine alignment of each magazine 10. The dewar 60 has a liquid cryogen, liquid nitrogen, inlet 88 on the side of the dewar 60. As shown in FIG. 12, five magazines 10 are placed in the working dewar 60, containing a total of sixty samples of crystals to be tested by x-ray crystallography.
  • Pin tongs [0026] 90 are part of the suite of the present invention since there are occasions when the cryo-pins 30 are handled manually.

Claims (20)

1. A magazine for storing and transferring batches of frozen mounted crystals on cryo-pins used in crystallography applications comprising:
a plurality of cylinders in which each cylinder a cryo-pin may be placed;
a location boss within each of said cylinders; and
a magnet centered with each boss for holding a cryo-pin within said cylinder.
2. A magazine according to claim 1 wherein an outer member surrounds said plurality of cylinders.
3. A magazine according to claim 1 wherein said cylinders are configured so that said outer member is essentially a circle.
4. A magazine according to claim 1 wherein said magazine has a top and a bottom, said bottom having said location bosses and a magnet on each said boss.
5. A magazine according to claim 1 wherein said outer member has a pair of tabs.
6. A magazine according to claim 4 wherein said magazine has twelve (12) cylinders
7. A worksite dewar for storing frozen mounted crystals in crystallography applications held in more than one magazine which comprises:
a flask having double-walls with a vacuum between the walls, said flask having a floor and wall, said floor having
a plurality of course alignment pins that match the exterior profile of said magazine, and
a plurality of fine alignment pins to precisely position said magazine on said floor; and
a top on said flask which may be opened and closed.
8. A worksite dewar according to claim 7 which has fine alignment pins for more than four magazines.
9. A worksite dewar according to claim 7 which has fine alignment pins for five (5) magazines.
10. A worksite dewar according to claim 7 wherein said top is opened and closed by a programmed controller.
11. A worksite dewar according to claim 7 which has a rim at the upper portion of said flask and a heater in the rim of said flask.
12. A worksite dewar for storing frozen mounted crystals in crystallography applications held in more than one magazine which comprises:
a flask having double-walls with a vacuum between the walls, said flask having a floor and wall, and a rim at the upper portion of said flask;
a top on said flask which may be opened and closed; and
a heater in the rim of said flask.
13. A worksite dewar according to claim 12 wherein said top is opened and closed by a programmed controller.
14. A worksite dewar according to claim 12 wherein said flask holds more than four magazines.
15. A worksite dewar according to claim 12 wherein said flask holds five magazines.
16. A worksite system used in crystallography applications comprising:
a dewar;
a plurality of magazines which may be placed in said dewar;
each magazine having a plurality of cylinders, each cylinder adapted to hold a cryo-pin having a crystal mounted thereon; and
a cryo-pin tong for removing said cryo-pin and positioning said crystal mounted on said pin in a goniometer.
17. A worksite system used in crystallography applications according to claim 16 wherein said dewar has a top that is opened and closed by a programmed controller.
18. A worksite system used in crystallography applications according to claim 16 wherein said dewar has a rim at the upper portion thereof and further includes a heater in said rim of said dewar.
19. A worksite system used in crystallography applications according to claim 17 wherein said dewar has a rim at the upper portion thereof and further includes
a heater in said rim of said dewar.
20. A worksite system used in crystallography applications comprising:
a dewar;
a programmed controller; and
a top on said dewar that is opened and closed by said programmed controller.
US10/349,234 2002-01-23 2003-01-22 Robot compatible crystal worksite suite Expired - Lifetime US6925815B2 (en)

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US20040187515A1 (en) * 2003-03-31 2004-09-30 Deming Shu Robot-based automation system for cryogenic crystal sample mounting
US20060086315A1 (en) * 2003-03-20 2006-04-27 Thorne Robert E Sample mounts for microcrystal crystallography
CN101482491B (en) * 2008-12-15 2011-11-02 中国科学院上海技术物理研究所 High background suppression type thermal infrared high-spectrum experimental device
US20130105677A1 (en) * 2011-10-28 2013-05-02 Fei Company Sample Block Holder
US20170161857A1 (en) * 2008-08-01 2017-06-08 Eamon Mason System and method for building multiple online legal research applications
JP2018519526A (en) * 2015-06-30 2018-07-19 イリノイ トゥール ワークス インコーポレイティド Inline X-ray measuring apparatus and method
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JP4648445B2 (en) * 2008-10-17 2011-03-09 大陽日酸株式会社 Cryopreservation device

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JP2018519526A (en) * 2015-06-30 2018-07-19 イリノイ トゥール ワークス インコーポレイティド Inline X-ray measuring apparatus and method
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JP2023511485A (en) * 2019-11-26 2023-03-20 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツング Sample holder and sample holder handling system for performing X-ray analysis on crystalline samples

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